本文選題：氮摻雜石墨烯 + 硫化物　； 參考：《安徽工業(yè)大學》2017年碩士論文

【摘要】：無酶修飾電極傳感器因其成本低、選擇性好、靈敏度高、檢測范圍寬等特點在生物電化學傳感器中成為近年來結(jié)合多學科且相互滲透的一項新興科技。葡萄糖、過氧化氫和亞硝酸鹽在醫(yī)藥和食品領域中是重要的分析檢測物。因此,采用新型的材料構(gòu)筑無酶電化學生物傳感器實現(xiàn)快速準確檢測其濃度成為研究熱點。自2004年發(fā)現(xiàn)機械剝離的石墨烯以來,因具有大的比表面積、高的導熱系數(shù)和快的載流子遷移率等優(yōu)良性質(zhì),而在各個領域的應用得到了廣泛地研究。但因其反應活性低,在電化學領域的應用受到局限。為了提高其電學性質(zhì),對其進行化學摻雜成為當前有效的無機化學方法。其中,氮摻雜石墨烯(N-graphene)因氮原子具有強失電子能力,能在碳原子周圍產(chǎn)生缺陷,提高了石墨烯的電催化活性而被進一步研究。本論文旨在運用N-graphene與硫基金屬納米材料進行復合,合成出一系列的N-graphene基納米復合材料,通過它們之間的協(xié)同作用提高其對葡萄糖、過氧化氫和亞硝酸鹽的電催化效果。論文主要內(nèi)容包括以下四方面:1.采用溶劑熱法探索合成了N-graphene與CoS_2納米材料形成的復合物,并對CoS_2/N-graphene復合納米材料修飾電極構(gòu)筑無酶葡萄糖傳感器進行研究。結(jié)果表明,與裸玻碳電極、N-graphene以及單一CoS_2納米材料修飾電極相比,CoS_2/N-graphene復合材料修飾電極對葡萄糖表現(xiàn)出最好的電催化效果,葡萄糖濃度在4μM~5.536 m M之間與其氧化峰電流呈良好的線性關(guān)系,靈敏度為421.75μA·m M~(-1)cm~(-2),檢出限達1.3μM。表明CoS_2/N-graphene復合材料充分發(fā)揮了各自單一材料的協(xié)同作用,從而對葡萄糖分子表現(xiàn)出顯著的催化活性。并且CoS_2/N-graphene復合材料修飾電極擁有良好的選擇性、穩(wěn)定性和重復性。這些優(yōu)越性能表明該復合材料有望發(fā)展成為在線檢測葡萄糖的電化學傳感器。2.探索合成了以粒子狀組成的海綿型的Co_4S_3納米材料,并將其與N-graphene結(jié)合形成納米復合材料。研究了H_2O_2分子在該復合材料修飾電極上的電化學響應。結(jié)果表明,與裸玻碳電極以及單一Co_4S_3材料修飾電極相比,Co_4S_3/N-graphene復合材料修飾電極對H_2O_2的電催化作用最強。運用安培法研究了Co_4S_3/N-graphene復合材料修飾電極對H_2O_2無酶傳感的線性范圍為:1μM~2.18 m M,檢測限為0.29μM,靈敏度為65.63μA/m M,響應時間為2 s。3.實驗中采用溶劑熱法合成Ni S/N-graphene復合材料,構(gòu)筑成葡萄糖無酶電化學傳感器后,通過環(huán)境友好的方式可靠、簡便地無酶化檢測葡萄糖。Ni S/N-graphene復合材料具有大的比表面積,并可作為電子傳遞介質(zhì),促進了電極和葡萄糖之間的電荷轉(zhuǎn)移,從而對葡萄糖的氧化表現(xiàn)出較強的電催化作用。當葡萄糖的濃度由5μM增至1.475 m M時安培響應曲線成線性增加。Ni S/N-graphene表現(xiàn)出來的寬的線性范圍、低的檢測限(1.7μM,S/N=3)、高的靈敏度(60.51μA·m M~(-1))和良好的選擇性等特點,為電化學傳感提供了一個良好的平臺。4.采用乙醇作溶劑合成了Cu S納米材料和Cu S/N-graphene納米復合材料,并對其進行必要的物相分析、形貌分析以及元素分析。采用循環(huán)伏安法探究Cu S/N-graphene納米復合材料對亞硝酸鹽的電催化效果。實驗結(jié)果表明,Cu S/N-graphene納米復合材料相對于Cu S納米材料的修飾電極,對亞硝酸鹽的氧化催化效果更強,氧化峰電流更高,氧化峰電位明顯負移。優(yōu)化各種實驗條件后發(fā)現(xiàn),亞硝酸鹽濃度在1μM~14.014 m M之間與其氧化峰電流呈良好的線性關(guān)系,檢出限達0.33μM。該復合材料修飾電極不受常見共存組分的干擾,并且重現(xiàn)性好,電極穩(wěn)定周期長,成功用于檢測實際樣品中的亞硝酸鹽。
[Abstract]:With low cost, good selectivity, high sensitivity and wide detection range, the non enzyme modified electrode sensor has become a new technology combining multidisciplinary and permeable in biosensors in recent years. Glucose, hydrogen peroxide and nitrite are important analytical agents in the field of medicine and food. Therefore, new methods are used in the field of Medicine and food. The rapid and accurate detection of its concentration has become a hot spot in the construction of an enzyme free electrochemical biosensor. Since the mechanical peeling of graphene in 2004, it has been widely studied in various fields because of its high specific surface area, high thermal conductivity and fast carrier mobility. In order to improve its electrical properties, chemical doping has become an effective inorganic chemical method in order to improve its electrical properties. In addition, nitrogen doped graphene (N-graphene) can produce defects around carbon atoms because of the strong electron loss ability of nitrogen atoms and improve the electrocatalytic activity of graphene. The purpose of this paper is to synthesize a series of N-graphene based nanocomposites by combining N-graphene with sulfur based metal nanomaterials, and to improve the electrocatalytic effect on glucose, hydrogen peroxide and nitrite by their synergism. The main contents of the thesis include the following four aspects: 1. the use of solvent heat The synthesis of N-graphene and CoS_2 nanocomposites was explored and the enzyme free glucose sensor was constructed on the CoS_2/N-graphene composite nanomaterial modified electrode. The results showed that the CoS_2/N-graphene composite modified electrode was compared with the naked glassy carbon electrode, N-graphene and the single CoS_2 Nanomaterial Modified electrode. The glucose showed the best electrocatalytic effect. The glucose concentration had a good linear relationship with the peak current of 4 M~5.536 m M, and the sensitivity was 421.75 A. M M~ (-1) cm~ (-2). The detection limit was 1.3 micron M. indicating that CoS_2/N-graphene composites fully played the synergistic effect of each single material, thus showing the glucose molecules. Significant catalytic activity. And the CoS_2/N-graphene composite modified electrode has good selectivity, stability and repeatability. These properties show that the composite is expected to develop into an electrochemical sensor for on-line detection of glucose and.2. to explore the synthesis of a particle like spongy Co_4S_3 nanomaterial, and N- The electrochemical response of H_2O_2 molecules on this composite modified electrode was studied by graphene. The results showed that the electrocatalysis of Co_4S_3/N-graphene composite modified electrode was the strongest compared with bare glassy carbon electrode and single Co_4S_3 modified electrode. Co_4S_3/N-gr was used to study Co_4S_3/N-gr by amperometric method. The linear range of the aphene composite modified electrode for H_2O_2 free enzyme sensing is 1 mu M~2.18 m M, the detection limit is 0.29 mu M, the sensitivity is 65.63 mu A/m M, and the response time is 2 s.3. experiment by solvent thermal synthesis of Ni S/N-graphene composite material, and after constructing the glucose free enzyme electrochemical sensor, it is reliable and simple by environmentally friendly way. The non enzymatic detection of glucose.Ni S/N-graphene composite has a large specific surface area, and can be used as an electron transfer medium, promoting the charge transfer between the electrode and glucose, thus showing a strong electrocatalytic effect on the oxidation of glucose. When the glucose concentration is increased from 5 to 1.475 m M, the ampere response curve is linearly increased. With the wide linear range, low detection limit (1.7, M, S/N=3), high sensitivity (60.51 A, m M~ (-1)) and good selectivity,.Ni S/N-graphene provides a good platform for electrochemical sensing with ethanol as solvent to synthesize Cu S nanomaterials and Cu nanocomposites. The necessary phase analysis, morphology analysis and elemental analysis are used to investigate the electrocatalytic effect of Cu S/N-graphene nanocomposites on nitrite by cyclic voltammetry. The experimental results show that the oxidation catalytic effect of Cu S/N-graphene nanocomposites is stronger than the modified electrode of Cu S nanomaterials, and the peak current of oxidation peak is higher. Higher oxidation peak potential is obviously negative. After optimizing the experimental conditions, it is found that the concentration of nitrite in 1 M~14.014 m M has a good linear relationship with the peak current of oxidation peak, and the detection limit is 0.33 M.. The composite modified electrode is not disturbed by common coexisting components, and it is highly repeatable, and the electrode has a long stable period and is successfully used for detection. Nitrite in the actual sample.

【學位授予單位】：安徽工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.1;TB332

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本文編號：1869062